QuEChERS结合超高效液相色谱-三重四极杆/线性离子阱串联质谱法同时测定食物中毒样品中的100种农药残留  

Determination of 100 pesticide residues in food poisoning samples by QuEChERS coupled with ultra-performance liquid chromatography-triple quadrupole/linear ion trap tandem mass spectrometry

作　　者：孙洁[1] 杨晓倩[1] 刘素华[1] 曹小丽[1] 焦海涛[1] 刘仲[1] SUN Jie;YANG Xiao-qian;LIU Su-hua;CAO Xiao-li;JIAO Hai-tao;LIU Zhong(Ji'nan Municipal Center for Disease Control and Prevention,Ji'nan,Shandong 250021,China)

机构地区：[1]济南市疾病预防控制中心,山东济南250021

出　　处：《中国卫生检验杂志》2020年第16期1921-1926,1931,共7页Chinese Journal of Health Laboratory Technology

基　　金：山东省医药卫生科技发展计划(2019WS070)。

摘　　要：目的建立食物中毒样品中100种农药残留的超高效液相色谱-三重四极杆/线性离子阱串联质谱的测定方法。方法样品经改进的QuEChERS方法提取和净化,ACQUITY UPLC BEH-C18柱(2.1 mm×100 mm,1.7μm)分离,0.1%甲酸水和乙腈为流动相梯度洗脱,采用多反应监测-信息相关采集-增强产物离子(MRM-IDA-EPI)扫描结合谱库检索进行分析,同时评估不同基质的基质效应以及不同吸附剂的净化效果。结果 100种农药的线性相关系数(r)均> 0.992 2,4种代表性基质(苹果、韭菜、孜然粉和猪肉)在3个加标水平(5μg/kg,20μg/kg和50μg/kg)的平均回收率为70.0%~119.2%,相对标准偏差为0.6%~17.0%。方法的检出限和定量限分别为0.01μg/kg^0.3μg/kg和0.03μg/kg^1.0μg/kg。结论该方法前处理简单、方便、准确、灵敏,适用于突发食物中毒事件中对农药残留的筛查和检测。Objective To establish a rapid analytical method for the simultaneous determination of 100 pesticides in food poisoning samples by an ultra-performance liquid chromatography-triple quadrupole/linear ion trap tandem mass spectrometry(UPLC-QTrap-MS/MS).Methods The food poisoning samples were extracted and purified with modified QuEChERS method.The 100 pesticides were separated using an ACQUITY UPLC BEH-C18 column(2.1 mm×100 mm,1.7μm)and gradient elution with the mobile phase consisting of 0.1%formic acid water and acetonitrile.A multiple reaction monitoring(MRM)scan as survey scan and an enhanced product ion(EPI)scan as dependent scan were performed in an information dependent acquisition(IDA)experiment.The matrix effects of different matrices and the purification effects of different adsorbents were evaluated.Results The calibration curves were linear(r>0.9922)for all the compounds.The mean recoveries for the 100 pesticides at three spiked levels(5μg/kg,20μg/kg,50μg/kg)and four different matrices(apple,leek,cumin powder and meat)were in the range of 70.0%-119.2%,with RSDs of 0.6%-17.0%.The limits of detection(LODs)and the limits of quantification(LOQs)for the 100 pesticides were within 0.01μg/kg-0.3μg/kg and 0.03μg/kg-1.0μg/kg.Conclusion The developed method is simple,rapid,sensitive,and it can be used for screening 100 kinds of pesticides residues in food poisoning samples.

关 键 词：食物中毒 农药残留 基质效应 QUECHERS 超高效液相色谱-三重四极杆/线性离子阱串联质谱 

分 类 号：O657.63[理学—分析化学]